Materials Science & Engineering A 822 (2021) 141633

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

The microstructure and high cycle fatigue performance of as-cast and

directionally solidified Ti46Al7Nb alloy under the three-point
bending loading
Xuesong Xu , Hongsheng Ding *, Wei Li , Haitao Huang , He Liang , Ruirun Chen , Jingjie Guo ,
Hengzhi Fu
National Key Laboratory for Precision Hot Processing of Metals, School of Materials Science and Engineering, Harbin Institute of Technology, Harbin, China

A R T I C L E I N F O A B S T R A C T

Keywords: This study systematically investigated the microstructure and high cycle fatigue deformation behavior of a high-
TiAl alloys Nb TiAl alloy with a nominal composition of Ti46Al7Nb alloy prepared by cold crucible directional solidification
Directional solidification (CCDS) method through TEM, SEM, etc. Macro/microstructure and phase component of as-cast and directionally
High cycle fatigue
solidified alloys were characterized. The three-point bending fatigue performance at room temperature was
Three-point bending
Fracture morphology
tested, and the corresponding fracture and deformation mechanisms were also revealed. Results show that the
Deformation mechanism columnar grains of the directionally solidified TiAl alloy are well-arranged in the direction of the heat flow.
Compared with the as-cast alloy, the segregation of the directionally solidified microstructure is significantly
improved. After 107 cycles, the three-point bending fatigue limit of the directionally solidified Ti46Al7Nb alloy is
about 60 MPa higher than that of the as-cast state. Fracture morphology shows that cleavage fracture is the main
fracture mode of the as-cast alloys. Quasi-cleavage fracture composed mainly of trans-lamellar fracture, sup­
plemented by small amount of plastic fracture, is the major fracture mode of directionally solidified Ti46Al7Nb
alloy. The fatigue deformation of this alloy mainly occurs in the γ lamellae. Dislocation multiplication and stress-
induced generation of subgrain are the main mechanisms of high cycle fatigue deformation of Ti46Al7Nb alloy.
Screw dislocations were also found in the γ subgrains generated after cyclic deformation. This research provides
a better understanding of the high cycle fatigue deformation of TiAl alloys.

1. Introduction range under the conditions of use, many researchers have been studying
the fatigue properties of TiAl alloys both at room temperature or high
TiAl-based intermetallic alloys have attracted considerable attention temperature [7–10]. Especially for the fully lamellar TiAl alloy with
for next-generation automotive and aerospace application due to their excellent resistance to crack growth, it is of great significance to inves­
low density, high specific strength and excellent high temperature tigate its performance under cyclic stress. Umakoshi and Nakano et al.
properties [1–3]. In particular, high-Nb containing TiAl alloys show [11,12] studied the deformation mechanism of poly-synthetically
even higher strength and oxidation resistance than ordinary TiAl alloy at twinned (PST) TiAl alloy under cyclic loading and pointed out that the
elevated temperatures [4–6]. anisotropy of the alloy has a significant effect on the fatigue life. Jha
By far the most anticipated engineering applications of TiAl alloys et al. [13] studied the fatigue performance of the fully-lamellar TiAl
involve components that are subjected to fluctuating or cyclic loading. It based alloy at room temperature and 600 ◦ C, and found that the fatigue
is essential to use fatigue test to evaluate the service life of TiAl alloys to life is the result of two fracture modes competing with each other, one is
simulate actual application conditions. The environment in which the failure by surface crack nucleation, the other is by subsurface crack
TiAl alloy is located should gradually increase from room temperature to nucleation. Under the action of cyclic loading, various forms of defor­
the applied high temperature and then stabilize, which means the ma­ mation behaviors will occur in TiAl alloys, including dislocation gen­
terial has been under cyclic load during the temperature change. In eration, twinning and phase transformation. Edwards et al. [14]
order to evaluate the performance of materials in the full temperature conducted a high cycle fatigue micro-compression test on lamellar TiAl

* Corresponding author.
E-mail address: [email protected] (H. Ding).

https://doi.org/10.1016/j.msea.2021.141633
Received 17 February 2021; Received in revised form 13 June 2021; Accepted 22 June 2021
Available online 24 June 2021
0921-5093/© 2021 Elsevier B.V. All rights reserved.
X. Xu et al. Materials Science & Engineering A 822 (2021) 141633

alloys, and found that small tightly arranged slip bands were generated revealed. Transmission electron microscope (TEM) was used to further
at the lamellar interface. Ding et al. [15] systematically studied the low study the deformation behavior of the alloy under cyclic loading, and
cycle fatigue deformation of high Nb-containing TiAl alloys at high the deformation mechanism of Ti46Al7Nb alloy was further discussed.
temperatures, and found that phase transformation of
α2lamellae→γ，α2+γ→B2(ω), and γ recrystallization widely occurred 2. Experiment procedures
during the cyclic deformations. Appel et al. [16] characterized the
microstructure of the high-Nb TiAl alloy after the low cycle fatigue test 2.1. Materials preparation
and found the phenomenon of stress-induced phase transformation of an
orthorhombic phase, which is apparently unstable under tetragonal A master ingot in this work with nominal composition of Ti46Al7Nb
distortion and transforms into fine γ lamellae. Park et al. [17] have (at. % hereinafter except the special illustration) and the size of ϕ100
observed the decomposition of lamellar structure and the occurrence of mm × 300 mm was prepared by induction skull melting furnace under
dynamic recrystallization processes, which are preferentially generated the protection of argon atmosphere. The raw materials were pure sponge
by deformation-induced heterogeneous nucleation at the titanium (99.9 wt %), pure aluminum (99.99 wt %), aluminum-75 wt %
sub-boundaries and proceeds by the nucleation of γ grains. Moreover, niobium master alloy. The actual average compositions of the ingots
there are a lot of work on the fatigue behavior of TiAl alloy under were examined by inductively coupled plasma atomic emission spec­
different stress states or temperature. C.L. Dong et al. [18] investigated trometry (ICPAES) method as Ti46.18Al7.22Nb. Feeder bars were cut
the effect of dwell time on fatigue life by carrying out the creep-fatigue from the master ingot into a cylinder bar with 20 mm in diameter and
interaction tests of a TiAl alloy at 750 ◦ C and 800 ◦ C in air, and proposed 300 mm in length by wire electrical discharge machining (EDM) for the
two life models based on dell time and minimum strain rate to predict following directional solidification experiment. The directional solidi­
low cycle fatigue life. S.P. Brookes et al. [19] investigated the uniaxial, fication of the master alloy was performed by electromagnetic cold
torsional and axial-torsional thermomechanical fatigue behavior of crucible directional solidification equipment (CCDS). The directional
near-γ TiAl alloy, and found the non-proportional multiaxial solidification process by electromagnetic cold crucible can be found
out-of-phase test showed a lower lifetime at the same equivalent me­ from previous study [34]. The CCDS experiment was carried out with
chanical strain amplitude compared to other types of tests. Q. Zhang the heating power of 55 kW and pulling rate of 16.7 μm/s under the
et al. [20] investigated the mean stress and phase angle effect on fatigue protection of high purity argon in the pressure of 300 Pa. The Ti46Al7Nb
behavior under combined tension-torsion fatigue loadings, and intro­ directional solidification ingot with the size of 26 × 26 × 120 mm.
duced a correction factor to make the modified prediction method
feasible for multiaxial fatigue life prediction with multiple loading 2.2. Microstructure characterization
variables. Current fatigue test research on TiAl alloy is mostly concen­
trated in the range of low cycle fatigue, which is mostly carried out The specimens were prepared by standard metallographic tech­
under tension or compression conditions. There are few studies on the niques and etched in the modified Kroll’s reagent of 5 vol%HF, 10 vol%
deformation behavior of TiAl alloys under transverse cyclic loading. HNO3 and 85 vol%H2O. Macrostructure is characterized by Nikon D850
In order to control the microstructure of TiAl alloys, electromagnetic Digital Single Lens Reflex. The microstructures of samples were inves­
cold crucible directional solidification technique has been widely used tigated by Quanta 200FEG (FEI, USA) scanning electron microscopy
in recent year [21–23], which can fabricate refractory and active alloys. (SEM) in backscattered electron (BSE). The phase constituents of the
The alloy is melted by electromagnetic induction heating, and is in soft ingots and samples were examined by X-ray diffraction (XRD) with Cu
contact with the water-cooled copper crucible under the action of Kα radiation using a Philip X-ray diffractometer, and the sample was
electromagnetic force, which avoids the possibility of reaction between scanned in a 2θ range of 20–90◦ with a speed of 2◦ min− 1. For the
the melt and the ceramic mold shell in the traditional Bridgman direc­ detailed analysis of the microstructures, the samples were further
tional solidification method. Due to the existence of a single direction of investigated by transmission electron microscope (TEM). TEM mea­
heat flow, a directional structure can be obtained by this method, and its surements were undertaken by a Talos F200X (FEI, USA) microscope.
performance is significantly improved [24,25]. Many researchers have The specimens for TEM observation were cut off from the deformation
studied the influence of lamellar orientation on mechanical properties of zone of samples after high cycle fatigue deformation by EDM and then
TiAl alloy, including tensile [26], fracture toughness [27], fatigue [28, ground to less than 50 μm manually. Finally, the ϕ3 mm foils were twin
29], etc., and the research results show that the fatigue performance is jet electron-polished in the solution of 60 vol% methanol, 35 vol%
highly correlated with the orientation of the lamellae. R. Gnanamoorthy butanol and 5 vol% perchloric acid at 30 V and − 25 ◦ C.
et al. [30] investigated the fatigue crack propagation behavior of TiAl
alloy with different lamellar orientation, and pointed out that the 2.3. Three-point bending fatigue test
lamellar lath at an angle to the crack plane produces high stress
shielding compared with the lamellar lath parallel to the crack plane. H. The equipment used for the three-point bending fatigue test is PLC-
Shiota et al. [31] also got a similar conclusion. In this paper, a cold 100C electromagnetic resonance fatigue testing machine (SINOTEST,
crucible directional solidification method is used to prepare TiAl alloy China). The maximum dynamic load is ±50 kN, and the loading fre­
with lamellar structure, which can effectively realize the control of the quency range is 80–250 Hz. The frequency of the equipment is deter­
lamellar orientation by changing the cooling rate [21], adjusting the mined by the cyclic load force parameters, sample size, etc., and the
alloy composition [32] and using seed crystal method [33], etc. Through frequency is adaptive. The span Ls of the sample used in the three-point
the preliminary experimental research, the corresponding relationship bending fatigue test is 28 mm, the cross-section is 6 × 6 mm, and the
between the optimal cooling rate and the lamellar orientation was diameter of the round bar of the applied and stressed indenter is 5 mm.
determined, and the directional solidification equipment was used to Since there is no special standard of the three-point bending fatigue test
prepare continuous lamellae with a 45◦ orientation to the growth di­ of metallic materials, this article refers to Metallic materials-Bend test
rection, which has the best combined effect of strength and plasticity (ISO 7438:2005) and Standard test method for fatigue crack growth
[34]. rates of metallic materials (GB/T 6398–2000) two standards to test the
In this study, the microstructure and phase component of Ti46Al7Nb three-point bending fatigue performance of this alloy. In order to avoid
alloy prepared by CCDS technique are studied compared with the as-cast the influence of the surface roughness of the sample on the fatigue
condition. The three-point bending high cycle fatigue tests of Ti46Al7Nb performance, the upper, lower and side surfaces are ground and pol­
alloy were carried out at room temperature. Through the observation of ished. At the same time, a kind of fixture was designed and processed
fracture morphology, the fracture mechanisms of the two-state alloy are independently in order to prevent the specimen from sliding during the

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X. Xu et al. Materials Science & Engineering A 822 (2021) 141633

cyclic load, as shown in Fig. 1. The fatigue limit is measured by a single diffuse. Fig. 3(b) shows the area enlarged by the yellow box in Fig. 3(a),
point method. When the stress amplitude is σ a,i, the number of cycles is from which it can be found that there are still a large number of
less than 10 million, and when the stress amplitude is σa,i+1, the number microcracks inside the lamellar colony. These microcracks are usually
of cycles is more than 10 million without fracture, if satisfied, distributed along the direction of the lamellar arrangement, which may
/ be caused by the phase transformation stress during the solidification of
(σ a,i − σa,i+1 ) σa,i+1 ≤ 5% (1)
the as-cast alloy.
/ Fig. 3(c) shows the microstructure of the directionally solidified
σ x = (σ a,i + σ a,i+1 ) 2 (2)
Ti46Al7Nb alloy. Its segregation has been significantly improved
compared with the as-cast alloy. The black segregation area disappears,
Where, σ a,i is the stress amplitude of the i-th time, and x is the stress
and the white segregation degree is reduced, which is attributed to the
ratio, the fatigue limit is σx.
fact that the alloy composition becomes very uniform at a result of the
electromagnetic stirring in the molten pool during the CCDS process. In
3. Results and analysis
addition, the slower solidification rate will also enable the alloy ele­
ments to diffuse effectively and reduce the effect of composition segre­
3.1. Macrostructure and microstructure
gation. Fig. 3(d) is the enlarged area of the yellow box in Fig. 3(c). It can
also be clearly seen that, compared with the as-cast alloy, there are
Fig. 2 shows the macrostructure of a directionally solidified high-Nb
basically no microcracks arranged along the lamellar direction, which
TiAl alloy ingot prepared by CCDS method. The macrostructure of the
attributes to the slow rate of directional solidification. The slower so­
directionally solidified Ti46Al7Nb alloy consists of three parts,
lidification rate means that the phase transition process can be fully
including the initial growth zone, the directionally solidified stable
carried out, thereby alleviating the adverse effects caused by the phase
growth zone and the final solidified zone. The initial growth zone is
transition stress. The grain size of the directionally solidified alloy is
produced when the directional solidification starts, the melting material
relatively large and the angle between lamellar orientation and growth
(usually the same as the directional solidification material or the seed
direction is approximately 45◦ . Even if there are two adjacent crystal
crystal that can play the role of seeding) is melted and thermally sta­
grains, the change of the lamellar orientation is not obvious.
bilized for a period of time. It creates conditions such as molten pool and
temperature gradient required for initial solidification for the stable
3.2. Phase component of Ti46Al7Nb alloys
growth of the directional solidification zone of TiAl alloy. The final so­
lidification zone is the structure formed when the cold crucible direc­
The phase component of the as-cast and directionally solidified
tional solidification ends, the ingot stops pulling and the power supply is
Ti46Al7Nb alloys is characterized by XRD patterns, as shown in Fig. 4. It
cut off, and finally the melt is naturally cooled. The columnar grains in
can be clearly found that the alloy is composed of α2 phase, γ phase and
this area are relatively fine and narrow, which is because the cooling
β0 phase, and the alloys in the two states show different diffraction peak
rate is faster than the slow pulling process of directional solidification.
distributions. The as-cast Ti46Al7Nb alloy has a large number of γ phase
The middle area of the ingot is a directionally solidified stable growth
diffraction peaks, indicating that the γ phase of the as-cast alloy can be
area. The columnar grains in this area are coarse and well-arranged
detected from different crystal planes, which means that its orientation
along the direction of heat flow.
distribution is relatively uniform. The number of diffraction peaks of
The microstructure of the as-cast and directionally solidified
directionally solidified alloy is less, but the intensity is higher than that
Ti46Al7Nb alloy is shown in Fig. 3. It can be seen that the as-cast and
of as-cast alloy, which implies the number of grains growing along a
directionally solidified high-Nb TiAl alloys are composed of lamellar
certain direction increases after directional solidification, while the
matrix and white network structure. Among them, the α2/γ lamellae
number of grains in other orientations decreases or disappears. This
matrix is obtained by the eutectoid transformation from α phase with
phenomenon indicates that CCDS can make the alloy grow in a specific
fixed Burgers orientation relationship, and the white network structure
direction while suppressing the grain growth of non-preferred orienta­
is the segregation phenomenon caused by the addition of β-stabilizing
tion. It is worth noting that no diffraction peak of β0 phase is found in the
element Nb. It can be found from Fig. 3(a) that the arrangement of the
directionally solidified Ti46Al7Nb alloy, which is caused by the weak­
lamellar colonies in the as-cast Ti46Al7Nb alloy is relatively messy, and
ening of the degree of segregation.
there are also black segregation zones inside the boundary of the
lamellar colonies apart from the white segregation, which is usually the
3.3. High cycle bending fatigue properties of Ti46Al7Nb alloys
place where Al is enriched. This is due to the uneven composition of the
as-cast Ti46Al7Nb alloy, and the relatively fast cooling rate leads to the
The stress levels and fatigue life of the three-point bending fatigue
serious segregation behavior caused by the element not having time to
test of the as-cast and directionally solidified Ti46Al7Nb alloys are
investigated systematically. The stress ratio of the three-point bending
fatigue test is all 0.1, that is, after loading to the maximum load,
unloading to 0.1 times the maximum load, and then cycling the stress
process. According to the results of Table 1, it can be concluded that with
the decrease of the stress level, the number of three-point bending fa­
tigue cycles of the alloy increases significantly, and the fatigue limit of
Ti46Al7Nb alloy in the two states is obtained. The relationship between
the maximum stress and the number of cycles of the as-cast and direc­
tionally solidified Ti46Al7Nb alloy is drawn (S–N curve), as shown in
Fig. 5. It can be concluded that the fatigue limit of the as-cast Ti46Al7Nb
alloy is 408 MPa, and the fatigue limit of the directionally solidified one
is 469 MPa based on the method in section 2.3. Comparing the above
results, the three-point bending fatigue performance of the directionally
solidified Ti46Al7Nb alloy has been significantly improved.

Fig. 1. Three-point bending high cycle fatigue test. (a) diagram of fatigue test
fixture; (b) specimen geometry for high cycle fatigue (HCF) testing.

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Fig. 2. Macrostructure of directionally solidified Ti46Al7Nb alloy prepared by CCDS.

4. Discussions

4.1. The crack initiation and propagation of Ti46Al7Nb alloy

High cycle three-point bending fatigue cracks originate from the

outer surface of the specimen in the bending direction. The specimen
adopts a three-point bending loading method, and the outer surface of
the bending specimen bears the maximum tensile stress, so fatigue
cracks are prone to initiation. From the perspective of microstructure,
cracks usually nucleate at the boundary of the lamellar structure or in
the γ phase. The TiAl alloy lamellar structure matrix is composed of
close-packed hexagonal α2 and face-centered square γ phase. The dif­
ference in the crystal structure of the two phases results in a different
number of movable slip systems, resulting in a different degree of co­
ordination of crystal deformation, which may produce a large coherent
stress between the two phases. When the stress concentration is large to
a certain degree, microcracks will be generated at the interface between
the two phases. In addition to the γ lamellae phase, the blocky γ phase
generated at the boundary of the lamellar colony may still produce
microcracks due to the different thermal expansion coefficient during
Fig. 3. Microstructure of Ti46Al7Nb alloy: (a) as-cast; (c) CCDS; (b) and (d) are the solidification process, which may also be the initiation of three-point
the enlarged yellow box of (a) and (c), respectively. (For interpretation of the bending fatigue cracks.
references to colour in this figure legend, the reader is referred to the Web Moreover, fatigue performance is highly correlated with the lamellar
version of this article.) orientation and boundary effect. It can be found that the angle between
lamellar orientation and directional growth direction is approximately
45◦ from Fig. 3, which has a good three-point bending fatigue resistance

Fig. 4. XRD pattern of as-cast and CCDS Ti46Al7Nb alloys.

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X. Xu et al. Materials Science & Engineering A 822 (2021) 141633

Table 1 states more likely to occur than the intragranular slip [35]. The crack is
Three-point bending fatigue test results of as-cast and CCDS TiAl alloys. blocked at the interface and the crack tip is blunt. Blocked cracks need to
No. Method stress f Stress Fatigue life N State increase the stress and tear the lamellar structure in a shearing manner
ratio (Hz) (MPa) (cycles) to further expand. Therefore, the interface acts as a hindrance to the
1 As-cast 0.1 83.8 405.23 10000128 No crack propagation process. (iii) The role of the grain boundary in the
failure crack propagation process is similar to that of the phase boundary. The
2 82.2 400.15 10000436 No interface is an irregular area of atomic arrangement, and the crystal
failure degree relationship on both sides is different. Therefore, the angle be­
3 84.3 395.89 12004388 No
failure
tween the arrangement direction and the crack propagation direction
4 82.5 379.93 11012143 No also determines whether it becomes an obstacle to crack propagation.
failure
5 85.2 410.83 4195773 failure
6 86.7 452.18 138829 failure 4.2. Fracture morphologies of Ti46Al7Nb alloys
7 85.9 411.77 724435 failure
8 85.1 499.9 35563 failure Fig. 6 shows the secondary electron (SE) image of the fracture
9 87.4 479.07 20734 failure
10 89.3 517.15 12058 failure
morphology of the as-cast Ti46Al7Nb alloy after three-point bending
11 CCDS 86.2 468.17 12005189 No fatigue test. It can be found that the three-point bending fatigue of the
failure as-cast Ti46Al7Nb alloy is a typical brittle cleavage fracture with inter-
12 85.6 466.01 10002483 No lamellar fracture as the main mode, supplemented by a small part of
failure
trans-lamellar fracture. There are a large number of fractured planes
13 84.9 460.79 10000396 No
failure along the lamellae and deeper cracks between the lamellar planes,
14 86.1 470.65 5330824 failure which are the results of the mutual peeling of the lamellae, as shown in
15 87.3 475.66 1835928 failure Fig. 6(a). Fig. 6(b) is an enlarged area of the yellow dashed frame in
16 87.1 483.33 919683 failure Fig. 6(a), from which it can be seen that the lamellar structure falls off
17 89.6 586.32 15576 failure
18 88.3 562.97 48016 failure
the substrate after the three-point bending cycle breaks to form a tearing
19 88.0 529.67 147892 failure edge. Fig. 6(c) shows the main characteristics of brittle cleavage fracture
20 88.7 523.01 226063 failure of as-cast Ti46Al7Nb alloy. Cleavage fracture is caused by the material
being cleaved strictly according to a certain crystallographic plane due
to the destruction of the bond between atoms under tensile stress. Fig. 6
(d) is the enlarged area of the yellow dashed frame in Fig. 6(c), from
which it can be seen that there are a series of cleavage planes arranged in
parallel to each other. The cleavage plane belongs to the low-index
crystal plane of the lamellar structure, which is because the low-index
plane has low surface energy and low theoretical fracture strength
[36,37]. Appel et al. [38] pointed out that the slip, twin and cleavage
plane of γ phase is {111} plane. Moreover, Yakovenkova et al. [39]
studied α2-Ti3Al single crystals to reveal that cleavage cracks tend to
occur on the (0001) basal plane. Accordingly, the traces of the
close-packed (111)γ and (0001)α2 planes, where cleavage fracture easily
occurs. Lu et al. [40] confirmed that the cleavage energy of the lamellar
interface is lower than that of the {111}γ plane. Thus, the crack tends to

Fig. 5. S–N curve of as-cast and CCDS Ti46Al7Nb alloys.

according to similar researches [28,30]. The lamellar interfaces and

grain boundaries will play the following roles in the process of crack
propagation: (i) When the lamellar interface arrangement direction is at
a small angle (less than 45◦ ) to the crack propagation direction, the
crack may propagate along the interface direction. The lamellar
boundary is usually a cleavage plane, which can act as a channel for
crack propagation. When the crack propagates along the cleavage plane
for a certain distance and deviates from the applied stress direction, it
will propagate through the lamellae perpendicular to the lamellar
arrangement direction at a small angle. (ii) When the lamellar interface
arrangement direction is at a large angle (more than 45◦ ) to the crack
propagation direction, the crack needs to extend through the interface.
There are differences in the crystal structure and crystal orientation
relationship on both sides of the lamellar phase interface, which can Fig. 6. Fracture morphology of the as-cast Ti46Al7Nb alloy after three-point
prevent slip bands and cleavage cracks from crossing the interface. In bending fatigue test. (a) and (c) are the fracture surfaces at different posi­
tions; (b) and (d) are the magnified images of the yellow dashed box in (a) and
addition, there are a large number of misfit dislocations at the lamella
(c), respectively. (For interpretation of the references to colour in this figure
phase interface, which makes the interface slip under certain stress
legend, the reader is referred to the Web version of this article.)

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propagate along the lamellar interface. The continuous distribution of

cleavage steps can also be observed, which are parallel to each other and
separated by the tearing edges.
Fig. 7 shows the three-point bending fatigue fracture morphology of
the directionally solidified Ti46Al7Nb alloy. Quasi-cleavage fracture
composed mainly of trans-lamellar fracture, supplemented by small
amount of plastic fracture, is the major fracture mode of directionally
solidified Ti46Al7Nb alloy. Fig. 7(a) shows the microstructure of
directionally solidified Ti46Al7Nb alloy with trans-lamellar fracture,
from which a large number of river patterns can be found, which is a
typical feature of brittle cleavage fracture. In addition, there are a large Fig. 8. Schematic diagram of quasi-cleavage fracture. (a) crack formation; (b)
crack propagation; (c) crack connected by tearing.
number of tearing edges that break through the lamellae, and a parallel
arrangement of lamellae can be found. Fig. 7(b) is an enlarged image of
the river pattern in Fig. 7(a). It can be seen that the direction of the river competition between dislocation emission against the cleavage separa­
expands from top to bottom, the upstream of the river is the origin of the tion at the crack tip [45,46]. The formation of the quasi-cleavage frac­
crack, and the downstream of the river is the direction of the crack ture morphology in this area may be due to the existence of a large
propagation. It can be judged that the crack expands from top to bottom number of tiny cleavage cracks in the material, which sprang up from
of the figure. Because the existence of boundaries hinders the movement various positions and continue to expand. The whole materials may be
of dislocations, dislocation plugging will occur at the interface and completely broken by plastic deformation tearing or dimple tearing at
induce cleavage cracks. Due to the disordered arrangement of atoms at the boundary where these cracks are connected to each other. Therefore,
the interface, the river cannot propagate through the grain boundary to the three-point bending fatigue performance of the directional solidified
the adjacent grain. Instead, new cleavage cracks are generated on the Ti46Al7Nb alloy is better than that of the as-cast alloy because its
grain boundary or in adjacent grains very close to the grain boundary, fracture mode changes from brittle cleavage fracture to quasi-cleavage
which expand outward in a fan-shaped manner and spread throughout fracture mode with a small amount of plastic deformation.
the entire grain. Fig. 7(c) shows the quasi-cleavage fracture morphology
observed in the directionally solidified Ti46Al7Nb alloy. It can be seen 4.3. Deformation behaviors of Ti46Al7Nb alloys during high cycle fatigue
that the morphology of the fracture not only has the cleavage fracture
characteristic, but also is accompanied by certain plastic fracture, which Fig. 9 are TEM images of Ti46Al7Nb alloy after three-point bending
can usually be observed in other materials [41–44]. Meanwhile, it can be high cycle fatigue cyclic deformation. It can be seen that the Ti46Al7Nb
observed that there are a large number of tearing edges on the alloy matrix is a fully-lamellar microstructure. Due to the high Al con­
quasi-cleavage plane, which are formed by the inter-connection of many tent of this alloy, the wider lamellae is the γ phase, and the narrower
separate cracks. Fig. 7(d) is an enlarged image of the area with plastic lamellae is the α2 phase. There are mainly two deformation behaviors
features in Fig. 7(c). Its fracture morphology is similar to that of dimples, found in the γ phase, one is the dislocation (the position marked by the
which is rarely observed in the brittle fracture process of TiAl alloys. red arrow), and the other is the subgrain produced by the stress-induced
Fig. 8 is a schematic diagram of quasi-cleavage fracture formation. phase transformation inside the γ lamellae (the position marked by the
For most engineering structural materials, microcracks can nucleate yellow arrow). Fig. 9(a) shows the deformed microstructure inside the
from the interface of phases, grains or between matrix and precipitates. as-cast Ti46Al7Nb alloy lamellae. It can be seen that there are a large
Also, α2/γ and γ/γ interface or inside the γ phase are potential nucleation
sites of microcracks, as shown in Fig. 3. After nucleation, whether the
microcracks will propagate in a cleavage or ductile mode depends on the

Fig. 7. Fracture morphology of the directionally solidified Ti46Al7Nb alloy Fig. 9. TEM image of Ti46Al7Nb alloy after three-point bending high cycle
after three-point bending fatigue test. (a) river-like pattern; (b) magnified image fatigue cyclic deformation. (a) as-cast; (b) CCDS; (c) stress-induced γ subgrain
of the yellow box in (a); (c) quasi-cleavage fracture morphology; (d) magnified (magnified image of the yellow box in (b)); (d) dislocation (magnified image of
image of the yellow box in (c). (For interpretation of the references to colour in the red box in (b)). (For interpretation of the references to colour in this figure
this figure legend, the reader is referred to the Web version of this article.) legend, the reader is referred to the Web version of this article.)

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number of dislocation lines of different lengths inside the lamellae, and dislocations, the remaining lattice mismatch can be accommodated
at the interface of the lamellae, the movement of dislocations is hindered uniformly by elastic strain, which leads to long-range coherent stress at
to produce dislocation packing. Meanwhile, the dislocation jog can be the interface [51]. The dislocation loop released from the interface can
found due to the interaction between forest dislocation and slipping prove the existence of coherent stress at the lamellar interface. The
dislocation, which is immobile and can serve as the short-range barrier position marked by the red arrow on the left in Fig. 9(d) is the dislo­
to the other dislocation movement. The yellow arrow marks are the cation loop released at the interface. Due to the geometric and crystal­
subgrains produced after the sample undergoes cyclic deformation, lographic limitations of the semi-coherent interface, the dislocation loop
which may be formed by the continuous coarsening of the lamellar cannot rotate around a fixed point [52]. As the deformation progresses,
structure in TiAl alloy [47,48]. Fig. 9(b) shows the morphology of the degree of the dislocation loop bowing out becomes more and more
lamellar deformation in the directionally solidified Ti46Al7Nb alloy. It serious, and the thread tension acting on the pinning point is greatly
is also obvious from the figure that there are a large number of dislo­ increased, which allows the dislocation loop to be easily released from
cations and subgrains in the lamellar structure, and the number of the semi-coherent interface and enter the interior of the γ lamellae [53].
subgrains is much higher than that of the as-cast alloy. By studying the Since coherent stress always exists at the semi-coherent interface, after
continuous coarsening mechanism of Ti–48Al alloy lamellae, Cao et al. the previous dislocation loop is released from the coherent interface, a
[49] showed that the continuous coarsening of the lamellar structure new dislocation loop will be formed. The dislocation loops at the
can not only be achieved by the migration of lamellar interface defects lamellar interface will be released from the interface under the action of
such as steps, ends and curved interfaces, but also by γ/γ interface applied shear stress to complete the dislocation multiplication. More­
migration or decomposition. Fig. 9(c) and (d) are the enlarged images in over, the dislocation lines released from the interface are tangled with
the yellow and red dashed boxes in Fig. 9(b), respectively. The γ/γ each other, resulting in obvious dislocation packing, as shown by the red
interface that ends in the γ lamellae appears, which can be speculated arrow in the middle of Fig. 9(d).
that the γ/γ interface migrates into the γ phase under the action of cyclic In order to further characterize the subgrain of Ti46Al7Nb alloy after
loading, leading to the generation of its subgrain, as shown in Fig. 9(c). high cycle fatigue deformation, TEM observation and analysis of the
Fig. 9(d) shows the dislocations in the γ lamellae. It can be seen that the subgrain appearing in the γ lamellae are carried out, as shown in Fig. 10.
dislocation lines are initiating from the phase interface. There is a Fig. 10(a) shows the bright field image after fatigue deformation of the
semi-coherent phase interface in the TiAl alloy lamellar structure, which directionally solidified Ti46Al7Nb alloy. It can be seen that a large
will lead to the existence of mismatch strain near the lamellar interface number of subgrains with different shapes are generated in the lamellar
[50]. Except for the partial strain mismatch accommodated by interface structure, some located independently inside the γ lamellae, some

Fig. 10. TEM and STEM image of the subgrain appearing in the γ lamellae. (a) bright-field image; (b) high-angle angular dark field (HAADF) image; (c)–(e) STEM
elemental maps of Ti46Al7Nb; (f) selected-area diffraction pattern of the interface of γ lamellae and newly generated subgrain (yellow circle marked in (a)); (g) dark-
field image of subgrain. (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)

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X. Xu et al. Materials Science & Engineering A 822 (2021) 141633

existing at the lamellar interface of γ/γ or γ/α2, and some dividing the γ is very straight and there is no obvious curvature change, continuous
lamellae into several parts. The high-angle angular dark field (HAADF) coarsening is usually difficult to occur. Due to the fatigue cyclic stress,
image and scanning transmission electron microscopy (STEM) elemental some interface defects will appear at the interface or inside of the γ
maps of the subgrain in the lamellae are shown in Fig. 10(b), (c), (d) and lamellae. According to Gibbs-Thomson theory [54–56],
(e). The content of Al element in the narrow lamellae is less, which can
Ce (r) = C(∞)exp(2γs Vm / rRT) (3)
be inferred to be α2 phase, while the element distribution in other po­
sitions is more uniform, which is γ lamellae. Inside the γ lamellae, where where, Ce(r) is the size dependence of equilibrium composition, γs is the
the subgrain exists, the distribution of the three elements does not interfacial energy density between the particle and matrix, Vm is the
change obviously, which can indicate that the element distribution and molar volume of the particle, R is the gas constant, T is the temperature,
content of the subgrain are consistent with the γ lamellae. The boundary and C (∞) is the equilibrium solute composition at the particle with the
position between the subgrain and the γ lamellar matrix is subjected to infinite size. As the deformation process progresses, the number of de­
selected area diffraction, and the result of the diffraction spot is shown in fects and the interface energy density gradually increase. Therefore, the
Fig. 10(f). It can be seen from the selected area diffraction results that equilibrium composition Ce(r) around the defects will increase on the
they are both γ phases, and share the same (200) crystal plane. Fig. 10(g) basis of Eq. (3). There will be a difference in solute concentration be­
is a dark field image of the subgrain in the γ lamellae. The dark field tween these defects and the flat interface. This concentration gradient
image shows the area that contributes to the intensity of the diffracted will result in a diffusion flow of solute atoms controlled by bulk diffusion
beam. It is further judged from the dark field image that the subgrain has between the defects and the flat interface, so that the interface defects
diffraction spots different from the γ lamellae. will migrate and cause the coarsening of the lamellae. In addition to
Fig. 11 shows the high-resolution TEM image between the subgrain relying on the migration of interface defects, the lamellar structure can
and the parent γ lamellae. Fig. 11(a) is a bright field image, indicating also be coarsened to produce subgrains through the migration or
the position taken by the HRTEM image, and Fig. 11(b) is the HRTEM decomposition of the γ/γ interface. The research results of Ramanujan
image magnified by the white box in Fig. 11(a). Enlarge the HRTEM et al. [47] and Miyazaki et al. [56] also confirmed the similar phe­
images of the three different positions in the γ lamellae matrix, the nomenon. As shown in Fig. 9(c), the generation of the subgrain is caused
subgrain and the γ lamellae interface, and the interior of the subgrain in by the decomposition and migration of the interface at the γ/γ phase
Fig. 11(b) to obtain Fig. 11(c), (d) and (e), respectively (marked with interface.
blue, yellow and red dashed box, respectively). Fig. 11(c) is a HRTEM Fig. 12 shows dislocations are both observed in the γ lamellae and
image of the interface between the γ lamellae matrix and the newly the newly generated γ subgrain after bending cyclic deformation. Fig. 12
formed subgrain, from which two different atomic arrangements can be (b) and (d) are the high-resolution images of the yellow and red dashed
observed, which is corresponding with the selected-area diffraction boxed in Fig. 12(a), respectively. From the diffraction spot patterns at
pattern in Fig. 10(f). According to the calculation of the interplanar the lower right corners of the two images obtained by Fast Fourier
spacing of the (001) plane and (200) plane of the γ lamellae in Fig. 11(d), Transform (FFT), it can be confirmed that the atomic arrangement lat­
they are 0.404 nm and 0.198 nm, respectively. The (110) crystal plane tice corresponds to the γ lamellae and the newly generated subgrain,
and (200) crystal plane spacing of the subgrain in Fig. 11(e) are 0.285 which is consistent with the results in Fig. 11. Fig. 12(c) is the area
nm and 0.198 nm, respectively. Therefore, the lattice constant was enlarged by the blue dashed box in Fig. 12(b). It can be clearly seen from
determined to be 3.962 Å of a and 4.031 Å of c, which was in agreement the figure that the γ phase, which is an ordered intermetallic compound,
with TiAl with a space group of P4/mmm (123) and a lattice constant of has very regular atomic arrangement. The darker area in the figure
3.976 Å of a and 4.049 Å of c (ICDD-PDF No. 05–0678 (2004)). Ac­ represents the position of the dislocation after deformation. It can be
cording to the above analysis, the newly generated subgrain belongs to γ clearly seen that the atoms in the area where the dislocation is located
phase, which has the same composition as the γ lamellar matrix but a and the matrix atoms have an obvious staggered arrangement, showing
different atomic arrangement. The formation of this γ subgrain may be obvious characteristics of screw dislocations. The position marked by
induced by three-point bending cyclic stress. Furthermore, because the the small red arrow in Fig. 12(c) is the result of a row of ordered atoms
coherent or semi-coherent interface in the TiAl alloy lamellar structure returning to the original order state after being misaligned through the

Fig. 11. TEM and high-resolution TEM (HRTEM) image of the interface between the γ lamellae and newly generated subgrain. (a) bright field image; (b) HRTEM
image of the interface and its Fast Fourier Transform (FFT) pattern (white box marked in (a)); (c), (d) and (e) are HRTEM images of the blue, yellow and red dashed
box in (b) and their FFT pattern, respectively. (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of
this article.)

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X. Xu et al. Materials Science & Engineering A 822 (2021) 141633

Fig. 12. Dislocations in the γ lamellae and the newly generated γ subgrain. (a) HAADF image; (b) dislocation in the γ lamellae (enlarged areas of yellow dashed box
in (a)); (c) is the enlarged area of blue dashed box in (b); (d) dislocation in the γ subgrain (enlarged areas of red dashed box in (a)); (e) and (f) enlarged areas of green
and pink dashed box in (d). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)

dislocation area. The atoms after passing through the staggered area still stress-induced γ phase to produce subgrains. In addition, screw
maintain the same arrangement pattern as the original arrangement dislocations can also be observed in both the γ lamellae and
direction. Furthermore, it can be found that there are several atom-sized subgrain.
vacancies in some positions (marked with yellow circles in (c) and (e)).
Fig. 12(e) and (f) are the enlarged areas of the green and pink dotted CRediT authorship contribution statement
boxes in Fig. 12(d), respectively. It can be observed that the arrange­
ment of the atomic array also shows obvious screw dislocation charac­ Xuesong Xu: Conceptualization, Investigation, Data curation,
teristics and some obvious vacancy defects. Fig. 12(f) is a high- Writing – original draft, Writing – review & editing. Hongsheng Ding:
resolution image at the boundary of the subgrain. This is the transi­ Supervision, Funding acquisition, Writing – review & editing. Wei Li:
tion region between the γ lamellae and the subgrain, from which it can Investigation, Resources. Haitao Huang: Supervision. He Liang:
be found that the atomic arrangement presents an obvious superlattice Investigation. Ruirun Chen: Supervision. Jingjie Guo: Supervision.
structure, and the atomic arrangement at the boundary where disloca­ Hengzhi Fu: Methodology.
tions are initiated is rather chaotic.

Declaration of competing interest

5. Conclusions

The authors declare that they have no known competing financial

In summary, the microstructure and high cycle fatigue performance
interests or personal relationships that could have appeared to influence
of directionally solidified Ti46Al7Nb alloy have been investigated
the work reported in this paper.
comparing with the as-cast condition. The main conclusions of this study
are as follows:
Acknowledgements
(1) Microstructural characterization shows that directionally solidi­
fied Ti46Al7Nb alloy show well-aligned columnar grains and less This work was supported by National Natural Science Foundation of
segregation than as-cast condition. China (Grant No. 51671072 and 51471062).
(2) Results of the three-point bending fatigue test show that after 107
cycles, the fatigue limit of the as-cast alloy is 408 MPa, and the References
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